CN105549152B - A kind of preparation method of the full sulphur system optical waveguide of Te base - Google Patents
A kind of preparation method of the full sulphur system optical waveguide of Te base Download PDFInfo
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- CN105549152B CN105549152B CN201610046599.1A CN201610046599A CN105549152B CN 105549152 B CN105549152 B CN 105549152B CN 201610046599 A CN201610046599 A CN 201610046599A CN 105549152 B CN105549152 B CN 105549152B
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/13—Integrated optical circuits characterised by the manufacturing method
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/13—Integrated optical circuits characterised by the manufacturing method
- G02B6/132—Integrated optical circuits characterised by the manufacturing method by deposition of thin films
Abstract
The invention discloses a kind of preparation methods of the full sulphur system optical waveguide of Te base comprising following steps: 1. taking one piece of chalcogenide glass as substrate；Then plating sets one layer of Ge-Sb-Se Chalcogenide films on the smooth upper surface of chalcogenide glass；Then a layer photoresist is coated on Ge-Sb-Se Chalcogenide films；2. 1. substrate that step obtains is exposed and is developed using the mask plate with required mask structure, the substrate with mask structure is obtained；3. plating sets one layer of Ge on the 2. substrate with mask structure that step obtains15Ga10Te75Chalcogenide films；4. 3. substrate that step is obtained is completely immersed in organic solvent, the photoresist in substrate 3. obtained using organic solvent dissolving step, while having taken away the Ge above photoresist15Ga10Te75Chalcogenide films form the full sulphur system optical waveguide of Te base；Advantage is that the full sulphur system optical waveguide of Te base that it is prepared has broader light through range, and has good confinement effect to light, can efficiently reduce transmission loss.
Description
Technical field
The present invention relates to a kind of technologies of preparing of optical waveguide, more particularly, to a kind of preparation side of the full sulphur system optical waveguide of Te base
Method.
Background technique
Integrated photon technology is the important development direction of photon technology.Optical waveguide is defined as being surrounded by region of low refractive index
The high-refractive-index regions got up, it is the basic composition unit of integrated optics and the basis of all optical communication.Planar integration light wave
Device is led since its miniaturization, integrated advantage are in the neck such as optical-fibre communications, optical remote sensing, sensing, optical storage and photoelectric display
Domain plays the effect to become more and more important.
Chalcogenide glass is to introduce Si (silicon), Ge (germanium), As based on chalcogen (S (sulphur), Se (selenium), Te (tellurium))
The amorphous material that the elements such as (arsenic), Sb (antimony) are formed, is a kind of infrared optical material, and there is high refractive index, high rare earth to mix for it
Miscellaneous ability, great optical nonlinearity and light sensitive characteristic, these features make chalcogenide glass fiber waveguide device infrared and remote in
Infrared-gas and bio-sensing, mid-infrared laser light source, all-optical device and interstellar space field of detecting have wide application
Prospect.Fig. 1 gives Te sill, Se sill, S sill, ZBLAN material and SiO2Material penetrates spectrum, from Fig. 1
It can be seen that Te sill it is infrared through window 20 microns near, and Se sill it is infrared transmission window it is attached at 17 microns
Closely, the infrared window that penetrates of S sill is near 13 microns.It can be seen that Te sill and Se sill, S in sulphur based material
Sill is compared, it has broader infrared transmission window (can achieve 25 microns), it can be completely covered bio-sensing and answer
Spectral region, in the fingerprint region of life detection, biological organism, detection is with a wide range of applications.
Current chalcogenide glass fiber waveguide device is substantially with SOI (Silicon-On-Insulator, in insulating substrate
Silicon) based on platform, substrate is the SiO of low-refraction2(silica) material, but due to SiO2The infrared cutoff wave of material
Length is less than 4 microns, therefore, mid and far infrared is transmitted, SiO is used2It necessarily will cause very big absorption loss as optical material,
This will affect the job applications of its infrared region.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of preparation methods of the full sulphur system optical waveguide of Te base, are prepared into
There is the full sulphur system optical waveguide of the Te base arrived broader light to penetrate range, and have good confinement effect to light, can be effectively
Reduce transmission loss.
The technical scheme of the invention to solve the technical problem is: a kind of preparation side of the full sulphur system optical waveguide of Te base
Method, it is characterised in that the following steps are included:
1. taking one piece of chalcogenide glass as substrate；Then plating sets one layer of Ge-Sb- on the smooth upper surface of chalcogenide glass
Se Chalcogenide films；Then a layer photoresist is coated on Ge-Sb-Se Chalcogenide films；
2. 1. substrate that step obtains is exposed and is developed using the mask plate with required mask structure, had
There is the substrate of mask structure；
3. plating sets one layer of Ge on the 2. substrate with mask structure that step obtains15Ga10Te75Chalcogenide films；
4. 3. substrate that step is obtained is completely immersed in organic solvent, the base 3. obtained using organic solvent dissolving step
Photoresist on material, while taking away the Ge above photoresist15Ga10Te75Chalcogenide films form the full sulphur system optical waveguide of Te base.
The step 1. in chalcogenide glass upper and lower surfaces be by polishing, polishing technology formed light
Sliding surface.
The step 1. on the smooth upper surface of chalcogenide glass plating set one layer of Ge-Sb-Se Chalcogenide films before,
First chalcogenide glass is cleaned to go deimpurity pollution, detailed process are as follows: 1. -1, by chalcogenide glass be completely immersed in acetone
In, it then utilizes ultrasonic cleaning 15 minutes~25 minutes, to remove the impurity on chalcogenide glass；1. -2, being taken out from acetone
Chalcogenide glass after cleaning for the first time, and the chalcogenide glass of taking-up is completely immersed in methanol, then divided using ultrasonic cleaning 3
Clock~8 minute, tentatively to remove remaining acetone on chalcogenide glass；1. -3, from the sulphur system taken out in methanol second after cleaning
Glass, and the chalcogenide glass of taking-up is completely immersed in isopropanol, it then utilizes ultrasonic cleaning 3 minutes~8 minutes, with complete
Remove remaining acetone on chalcogenide glass；1. the chalcogenide glass cleaned up -4, is taken out from isopropanol, then with being dried with nitrogen
The chalcogenide glass cleaned up.Here, the impurity on chalcogenide glass is effectively removed first with acetone, it is then preliminary using methanol
Remaining acetone on chalcogenide glass is removed, isopropanol is recycled to completely remove remaining acetone on chalcogenide glass, finally drying is clear
The chalcogenide glass of wash clean, carrying out cleaning treatment to the surface of chalcogenide glass can be such that subsequent waveguide preparation process flow keeps
Completely.
The step 1. in the platings of Ge-Sb-Se Chalcogenide films set using magnetically controlled sputter method, wherein magnetron sputtering
The vacuum degree of the sputtering chamber of membranous system is 1.5 × 10-4Pa~2.5 × 10-4Pa, build-up of luminance air pressure are 2.8 pas~3.2 pas, magnetic control
The sputtering pressure of sputter coating system is 0.22 pa~0.27 pa, sputtering power is 25 watts~30 watts, sputtering time is 2 small
When~3 hours, the volume flow for the argon gas being passed through into the sputtering chamber of magnetron sputtering coating system is 45sccm~55sccm.
Here, setting the Ge-Sb-Se Chalcogenide films that Ge-Sb-Se Chalcogenide films enable to using the plating of existing magnetically controlled sputter method
Uniformity is good, and compositional difference is small；And the parameter of work is sputtered by limiting magnetron sputtering coating system, the Ge- obtained can be made
Sb-Se Chalcogenide films have the characteristics that compactness is good, optical scattering losses are small, uniformity is good, are suitble to the production of planar optical waveguide.
The step 1. in photoresist coating utilize sol evenning machine, wherein fast-turn construction after the slow-speed of sol evenning machine elder generation, slow-speed revolving speed
For 2000rpm, the slow-speed time is 3 seconds, and fast-turn construction revolving speed is 6000rpm, and the fast-turn construction time is 30 seconds.Here, coating photoresist is first slow
Fast-turn construction can make photoresist adherency good and uniform after turning.
The step 1. in Ge-Sb-Se Chalcogenide films with a thickness of 0.8~1.2 micron, photoresist with a thickness of
1.5~1.8 microns.Here, limit Ge-Sb-Se Chalcogenide films thickness be in order to reduce Ge-Sb-Se Chalcogenide films and
Ge15Ga10Te75Stress between Chalcogenide films；Limit photoresist thickness be greater than Ge-Sb-Se Chalcogenide films thickness be in order to
Prepare sulphur system optical waveguide smooth.
The detailed process of the step 2. are as follows: 2. -1, using contact system, be close to what 1. step obtained in mask plate
1. substrate that step obtains is exposed after photoresist in substrate, wherein the time for exposure is 8 seconds~12 seconds；2. -2, in hydrogen
Develop in sodium oxide molybdena alkaline-based developer to the substrate after exposure, obtains the substrate with mask structure, wherein developing time
It is 45 seconds~60 seconds.Here, limiting the time for exposure is to generate a good figure on the substrate for have been coated with photoresist；
Limiting developing time is in order to which the figure of mask plate is accurately copied in photoresist, to guarantee the quality of photoetching.
The step 3. in Ge15Ga10Te75The plating of Chalcogenide films is set using magnetically controlled sputter method, wherein magnetron sputtering
The vacuum degree of the sputtering chamber of coating system is 1.5 × 10-4Pa~2.5 × 10-4Pa, build-up of luminance air pressure are 2.8 pas~3.2 pas, magnetic
The sputtering pressure for controlling sputter coating system is 0.22 pa~0.27 pa, sputtering power is 25 watts~30 watts, sputtering time 2
Hour~3 hours, the volume flow of the argon gas being passed through into the sputtering chamber of magnetron sputtering coating system be 45sccm~
55sccm.Here, setting Ge using the plating of existing magnetically controlled sputter method15Ga10Te75What Chalcogenide films enabled to
Ge15Ga10Te75The uniformity of Chalcogenide films is good, and compositional difference is small；And work is sputtered by limiting magnetron sputtering coating system
Parameter so that obtain Ge15Ga10Te75Chalcogenide films have the characteristics that compactness is good, optical scattering losses are small, uniformity is good,
It is suitble to the production of planar optical waveguide.
The step 3. in Ge15Ga10Te75Chalcogenide films with a thickness of 0.8~1.2 micron.Here, limiting
Ge15Ga10Te75The thickness of Chalcogenide films is the height in order to obtain required optical waveguide.
Photoresist on the step substrate that 4. 3. middle utilization organic solvent dissolving step obtains, while taking away and being located at
Ge above photoresist15Ga10Te75It is recycled ultrasonic cleaning 5 minutes~10 minutes after Chalcogenide films；The step 4. in
Organic solvent be N-Methyl pyrrolidone that concentration is 99.9%.Here, carrying out ultrasonic cleaning when dissolving photoresist is
In order to come into full contact with photoresist and organic solvent, thus the structure of optical waveguide required for obtaining；Use concentration for 99.9%
N-Methyl pyrrolidone can effectively dissolve the photoresist on substrate, while also having taken away above photoresist
Ge15Ga10Te75Chalcogenide films.
Compared with the prior art, the advantages of the present invention are as follows:
1) the method for the present invention is using selenide thin film as substrate material, and tellurides film is light function transmission material, and existing
SiO2Material is compared, and tellurides thin-film material has broader light through range (long wave cut-off wavelength reachable~15 microns),
The absorption of infrared light can be effectively reduced.
2) the method for the present invention is using selenide thin film and tellurides film as waveguiding structure material, due to selenides and telluro
Material belongs to same family, and material property is close, therefore can be effectively reduced when waveguide photoetching makes annealing treatment because of the coefficient of expansion
Film layer break-off caused by difference.
Detailed description of the invention
Fig. 1 is Te material, Se sill, S sill, ZBLAN material and SiO2Material penetrates spectrum；
Fig. 2 is the Ge measured using infrared ellipsometer24Sb3Se73Chalcogenide films and Ge15Ga10Te75Chalcogenide films are respective
The relation curve of refractive index and wavelength；
Fig. 3 is the result schematic diagram in per stage during preparing the full sulphur system optical waveguide of Te base using the method for the present invention；
Fig. 4 is the cross-sectional view for the full sulphur system optical waveguide structure of Te base that embodiment one is prepared；
Fig. 5 a is to carry out emulation experiment in wavelength to the full sulphur system optical waveguide of Te base shown in Fig. 4 using existing simulation software
For the mode distributions figure for simulating obtained TE mould at 4.8 microns；
Fig. 5 b is to carry out emulation experiment in wavelength to the full sulphur system optical waveguide of Te base shown in Fig. 4 using existing simulation software
For the mode distributions figure for simulating obtained TM mould at 4.8 microns.
Specific embodiment
Closing figure embodiment below, present invention is further described in detail.
Embodiment one:
A kind of preparation method for the full sulphur system optical waveguide of Te base that the present embodiment proposes comprising following steps:
1. a block size is taken to be divided into Ge for 0.1 centimetre of 3 cm x, 3 cm x, group20Sb15Se65Chalcogenide glass (Chg) make
For substrate, the upper and lower surfaces of the chalcogenide glass be by polishing, the smooth surface that polishing technology is formed；Then exist
Plating sets a layer thickness as 1.2 microns of Ge on the smooth upper surface of chalcogenide glass24Sb3Se73Chalcogenide films；Followed by existing
Sol evenning machine in Ge24Sb3Se73The photoresist that a layer thickness is 1.5 microns is coated on Chalcogenide films.
In this particular embodiment, plating sets one layer of Ge on the smooth upper surface of chalcogenide glass24Sb3Se73Chalcogenide films
Before, first chalcogenide glass is cleaned to go deimpurity pollution, detailed process are as follows: 1. -1, by chalcogenide glass be completely immersed in
In acetone, then utilize ultrasonic cleaning 20 minutes, to remove the impurity on chalcogenide glass；1. -2, taking out first from acetone
Chalcogenide glass after secondary cleaning, and the chalcogenide glass of taking-up is completely immersed in methanol, then utilize ultrasonic cleaning 5 minutes,
Tentatively to remove remaining acetone on chalcogenide glass；1. -3, from the chalcogenide glass taken out in methanol second after cleaning, and will take
Chalcogenide glass out is completely immersed in isopropanol, is then utilized ultrasonic cleaning 5 minutes, is remained on chalcogenide glass with completely removing
Acetone；1. the chalcogenide glass cleaned up -4, is taken out from isopropanol, then with being dried with nitrogen the sulphur system glass cleaned up
Glass.
In this particular embodiment, Ge24Sb3Se73The plating of Chalcogenide films is set using existing magnetically controlled sputter method, wherein
The vacuum degree of the sputtering chamber of magnetron sputtering coating system is 2.0 × 10-4Pa, build-up of luminance air pressure are 3 pas, magnetron sputtering coating system
Sputtering pressure be 0.25 pa, sputtering power is 30 watts, sputtering time is 2 hours, the sputtering to magnetron sputtering coating system
The volume flow for the argon gas being passed through in chamber is 50sccm.
In this particular embodiment, the coating of photoresist utilizes existing sol evenning machine, wherein fast after the slow-speed of sol evenning machine elder generation
Turn, slow-speed revolving speed is 2000rpm, and the slow-speed time is 3 seconds, and fast-turn construction revolving speed is 6000rpm, and the fast-turn construction time is 30 seconds.
In this particular embodiment, photoresist uses AZ5214 photoresist.
2. 1. substrate that step obtains is exposed and is developed using the mask plate with required mask structure, had
There is the substrate of mask structure.Photoetching is an important factor for influencing photonic device quality, on the one hand it determines optical waveguide
The attainable size of institute, on the other hand determines the quality of optical waveguide line quality.
In this particular embodiment, the detailed process of step 2. are as follows: 2. -1, using existing contact system, in exposure mask
Plate is exposed 1. substrate that step obtains after being close to the photoresist in the substrate that 1. obtains of step, wherein the time for exposure is
10 seconds；2. -2, developing in Sodium Hydroxide Alkaline developer solution to the substrate after exposure, the base with mask structure is obtained
Material, wherein developing time is 50 seconds.
3. plating sets a layer thickness as 1 micron of Ge on the 2. substrate with mask structure that step obtains15Ga10Te75Sulphur
It is film.
In this particular embodiment, Ge15Ga10Te75The plating of Chalcogenide films is set using existing magnetically controlled sputter method, wherein
The vacuum degree of the sputtering chamber of magnetron sputtering coating system is 2.0 × 10-4Pa, build-up of luminance air pressure are 3 pas, magnetron sputtering coating system
Sputtering pressure be 0.25 pa, sputtering power is 30 watts, sputtering time is 2 hours, the sputtering to magnetron sputtering coating system
The volume flow for the argon gas being passed through in chamber is 50sccm.
4. 3. substrate that step is obtained is completely immersed in organic solvent, the base 3. obtained using organic solvent dissolving step
Photoresist on material, while also having taken away the Ge above photoresist15Ga10Te75When Chalcogenide films, recycle ultrasonic wave clear
It washes 10 minutes, forms the full sulphur system optical waveguide of Te base.
In this particular embodiment, organic solvent is the N-Methyl pyrrolidone that concentration is 99.9%.
Embodiment two:
A kind of preparation method for the full sulphur system optical waveguide of Te base that the present embodiment proposes comprising following steps:
1. a block size is taken to be divided into Ge for 0.1 centimetre of 3 cm x, 3 cm x, group20Sb15Se65Chalcogenide glass (Chg) make
For substrate, the upper and lower surfaces of the chalcogenide glass be by polishing, the smooth surface that polishing technology is formed；Then exist
Plating sets a layer thickness as 1 micron of Ge on the smooth upper surface of chalcogenide glass24Sb3Se73Chalcogenide films；Followed by existing
Sol evenning machine is in Ge24Sb3Se73The photoresist that a layer thickness is 1.8 microns is coated on Chalcogenide films.
In this particular embodiment, plating sets one layer of Ge on the smooth upper surface of chalcogenide glass24Sb3Se73Chalcogenide films
Before, first chalcogenide glass is cleaned to go deimpurity pollution, detailed process are as follows: 1. -1, by chalcogenide glass be completely immersed in
In acetone, then utilize ultrasonic cleaning 18 minutes, to remove the impurity on chalcogenide glass；1. -2, taking out first from acetone
Chalcogenide glass after secondary cleaning, and the chalcogenide glass of taking-up is completely immersed in methanol, then utilize ultrasonic cleaning 8 minutes,
Tentatively to remove remaining acetone on chalcogenide glass；1. -3, from the chalcogenide glass taken out in methanol second after cleaning, and will take
Chalcogenide glass out is completely immersed in isopropanol, is then utilized ultrasonic cleaning 6 minutes, is remained on chalcogenide glass with completely removing
Acetone；1. the chalcogenide glass cleaned up -4, is taken out from isopropanol, then with being dried with nitrogen the sulphur system glass cleaned up
Glass.
In this particular embodiment, Ge24Sb3Se73The plating of Chalcogenide films is set using existing magnetically controlled sputter method, wherein
The vacuum degree of the sputtering chamber of magnetron sputtering coating system is 1.8 × 10-4Pa, build-up of luminance air pressure are 3.2 pas, magnetron sputtering membrane system
The sputtering pressure of system is 0.22 pa, sputtering power is 25 watts, sputtering time is 3 hours, to splashing for magnetron sputtering coating system
The volume flow for penetrating the argon gas being passed through in chamber is 52sccm.
In this particular embodiment, the coating of photoresist utilizes existing sol evenning machine, wherein fast after the slow-speed of sol evenning machine elder generation
Turn, slow-speed revolving speed is 2000rpm, and the slow-speed time is 3 seconds, and fast-turn construction revolving speed is 6000rpm, and the fast-turn construction time is 30 seconds.
In this particular embodiment, photoresist uses AZ5214 photoresist.
2. 1. substrate that step obtains is exposed and is developed using the mask plate with required mask structure, had
There is the substrate of mask structure.Photoetching is an important factor for influencing photonic device quality, on the one hand it determines optical waveguide
The attainable size of institute, on the other hand determines the quality of optical waveguide line quality.
In this particular embodiment, the detailed process of step 2. are as follows: 2. -1, using existing contact system, in exposure mask
Plate is exposed 1. substrate that step obtains after being close to the photoresist in 1. substrate that step obtains, wherein the time for exposure 8
Second；2. -2, developing in Sodium Hydroxide Alkaline developer solution to the substrate after exposure, the substrate with mask structure is obtained,
Wherein, developing time is 45 seconds.
3. plating sets a layer thickness as 0.8 micron of Ge on the 2. substrate with mask structure that step obtains15Ga10Te75
Chalcogenide films.
In this particular embodiment, Ge15Ga10Te75The plating of Chalcogenide films is set using existing magnetically controlled sputter method, wherein
The vacuum degree of the sputtering chamber of magnetron sputtering coating system is 1.8 × 10-4Pa, build-up of luminance air pressure are 3.2 pas, magnetron sputtering membrane system
The sputtering pressure of system is 0.22 pa, sputtering power is 25 watts, sputtering time is 3 hours, to splashing for magnetron sputtering coating system
The volume flow for penetrating the argon gas being passed through in chamber is 52sccm.
4. 3. substrate that step is obtained is completely immersed in organic solvent, the base 3. obtained using organic solvent dissolving step
Photoresist on material, while also having taken away the Ge above photoresist15Ga10Te75When Chalcogenide films, recycle ultrasonic wave clear
It washes 8 minutes, forms the full sulphur system optical waveguide of Te base.
In this particular embodiment, organic solvent is the N-Methyl pyrrolidone that concentration is 99.9%.
Embodiment three:
A kind of preparation method for the full sulphur system optical waveguide of Te base that the present embodiment proposes comprising following steps:
1. a block size is taken to be divided into Ge for 0.1 centimetre of 3 cm x, 3 cm x, group28Sb12Se60Chalcogenide glass (Chg) make
For substrate, the upper and lower surfaces of the chalcogenide glass be by polishing, the smooth surface that polishing technology is formed；Then exist
Plating sets a layer thickness as 1.2 microns of Ge on the smooth upper surface of chalcogenide glass20Sb15Se65Chalcogenide films；Followed by existing
Some sol evenning machines are in Ge20Sb15Se65The photoresist that a layer thickness is 1.5 microns is coated on Chalcogenide films.
In this particular embodiment, plating sets one layer of Ge on the smooth upper surface of chalcogenide glass20Sb15Se65Chalcogenide films
Before, first chalcogenide glass is cleaned to go deimpurity pollution, detailed process are as follows: 1. -1, by chalcogenide glass be completely immersed in
In acetone, then utilize ultrasonic cleaning 25 minutes, to remove the impurity on chalcogenide glass；1. -2, taking out first from acetone
Chalcogenide glass after secondary cleaning, and the chalcogenide glass of taking-up is completely immersed in methanol, then utilize ultrasonic cleaning 4 minutes,
Tentatively to remove remaining acetone on chalcogenide glass；1. -3, from the chalcogenide glass taken out in methanol second after cleaning, and will take
Chalcogenide glass out is completely immersed in isopropanol, is then utilized ultrasonic cleaning 8 minutes, is remained on chalcogenide glass with completely removing
Acetone；1. the chalcogenide glass cleaned up -4, is taken out from isopropanol, then with being dried with nitrogen the sulphur system glass cleaned up
Glass.
In this particular embodiment, Ge20Sb15Se65The plating of Chalcogenide films is set using existing magnetically controlled sputter method, wherein
The vacuum degree of the sputtering chamber of magnetron sputtering coating system is 2.5 × 10-4Pa, build-up of luminance air pressure are 2.8 pas, magnetron sputtering membrane system
The sputtering pressure of system is 0.27 pa, sputtering power is 27 watts, sputtering time is 2.5 hours, to magnetron sputtering coating system
The volume flow for the argon gas being passed through in sputtering chamber is 45sccm.
In this particular embodiment, the coating of photoresist utilizes existing sol evenning machine, wherein fast after the slow-speed of sol evenning machine elder generation
Turn, slow-speed revolving speed is 2000rpm, and the slow-speed time is 3 seconds, and fast-turn construction revolving speed is 6000rpm, and the fast-turn construction time is 30 seconds.
In this particular embodiment, photoresist uses AZ5214 photoresist.
2. 1. substrate that step obtains is exposed and is developed using the mask plate with required mask structure, had
There is the substrate of mask structure.Photoetching is an important factor for influencing photonic device quality, on the one hand it determines optical waveguide
The attainable size of institute, on the other hand determines the quality of optical waveguide line quality.
In this particular embodiment, the detailed process of step 2. are as follows: 2. -1, using existing contact system, in exposure mask
Plate is exposed 1. substrate that step obtains after being close to the photoresist in the substrate that 1. obtains of step, wherein the time for exposure is
12 seconds；2. -2, developing in Sodium Hydroxide Alkaline developer solution to the substrate after exposure, the base with mask structure is obtained
Material, wherein developing time is 45 seconds.
3. plating sets a layer thickness as 1 micron of Ge on the 2. substrate with mask structure that step obtains15Ga10Te75Sulphur
It is film.
In this particular embodiment, Ge15Ga10Te75The plating of Chalcogenide films is set using existing magnetically controlled sputter method, wherein
The vacuum degree of the sputtering chamber of magnetron sputtering coating system is 2.5 × 10-4Pa, build-up of luminance air pressure are 2.8 pas, magnetron sputtering membrane system
The sputtering pressure of system is 0.27 pa, sputtering power is 27 watts, sputtering time is 2.5 hours, to magnetron sputtering coating system
The volume flow for the argon gas being passed through in sputtering chamber is 45sccm.
4. 3. substrate that step is obtained is completely immersed in organic solvent, the base 3. obtained using organic solvent dissolving step
Photoresist on material, while also having taken away the Ge above photoresist15Ga10Te75When Chalcogenide films, recycle ultrasonic wave clear
It washes 6 minutes, forms the full sulphur system optical waveguide of Te base.
In this particular embodiment, organic solvent is the N-Methyl pyrrolidone that concentration is 99.9%.
Example IV:
A kind of preparation method for the full sulphur system optical waveguide of Te base that the present embodiment proposes comprising following steps:
1. a block size is taken to be divided into Ge for 0.1 centimetre of 3 cm x, 3 cm x, group28Sb12Se60Chalcogenide glass (Chg) make
For substrate, the upper and lower surfaces of the chalcogenide glass be by polishing, the smooth surface that polishing technology is formed；Then exist
Plating sets a layer thickness as 1 micron of Ge on the smooth upper surface of chalcogenide glass20Sb15Se65Chalcogenide films；Followed by existing
Sol evenning machine in Ge20Sb15Se65The photoresist that a layer thickness is 1.8 microns is coated on Chalcogenide films.
In this particular embodiment, plating sets one layer of Ge on the smooth upper surface of chalcogenide glass20Sb15Se65Chalcogenide films
Before, first chalcogenide glass is cleaned to go deimpurity pollution, detailed process are as follows: 1. -1, by chalcogenide glass be completely immersed in
In acetone, then utilize ultrasonic cleaning 25 minutes, to remove the impurity on chalcogenide glass；1. -2, taking out first from acetone
Chalcogenide glass after secondary cleaning, and the chalcogenide glass of taking-up is completely immersed in methanol, then utilize ultrasonic cleaning 4 minutes,
Tentatively to remove remaining acetone on chalcogenide glass；1. -3, from the chalcogenide glass taken out in methanol second after cleaning, and will take
Chalcogenide glass out is completely immersed in isopropanol, is then utilized ultrasonic cleaning 8 minutes, is remained on chalcogenide glass with completely removing
Acetone；1. the chalcogenide glass cleaned up -4, is taken out from isopropanol, then with being dried with nitrogen the sulphur system glass cleaned up
Glass.
In this particular embodiment, Ge20Sb15Se65The plating of Chalcogenide films is set using existing magnetically controlled sputter method, wherein
The vacuum degree of the sputtering chamber of magnetron sputtering coating system is 2.5 × 10-4Pa, build-up of luminance air pressure are 2.8 pas, magnetron sputtering membrane system
The sputtering pressure of system is 0.27 pa, sputtering power is 27 watts, sputtering time is 2.5 hours, to magnetron sputtering coating system
The volume flow for the argon gas being passed through in sputtering chamber is 45sccm.
In this particular embodiment, the coating of photoresist utilizes existing sol evenning machine, wherein fast after the slow-speed of sol evenning machine elder generation
Turn, slow-speed revolving speed is 2000rpm, and the slow-speed time is 3 seconds, and fast-turn construction revolving speed is 6000rpm, and the fast-turn construction time is 30 seconds.
In this particular embodiment, photoresist uses AZ5214 photoresist.
2. 1. substrate that step obtains is exposed and is developed using the mask plate with required mask structure, had
There is the substrate of mask structure.Photoetching is an important factor for influencing photonic device quality, on the one hand it determines optical waveguide
The attainable size of institute, on the other hand determines the quality of optical waveguide line quality.
In this particular embodiment, the detailed process of step 2. are as follows: 2. -1, using existing contact system, in exposure mask
Plate is exposed 1. substrate that step obtains after being close to the photoresist in the substrate that 1. obtains of step, wherein the time for exposure is
12 seconds；2. -2, developing in Sodium Hydroxide Alkaline developer solution to the substrate after exposure, the base with mask structure is obtained
Material, wherein developing time is 45 seconds.
3. plating sets a layer thickness as 0.8 micron of Ge on the 2. substrate with mask structure that step obtains15Ga10Te75
Chalcogenide films.
In this particular embodiment, Ge15Ga10Te75The plating of Chalcogenide films is set using existing magnetically controlled sputter method, wherein
The vacuum degree of the sputtering chamber of magnetron sputtering coating system is 2.5 × 10-4Pa, build-up of luminance air pressure are 2.8 pas, magnetron sputtering membrane system
The sputtering pressure of system is 0.27 pa, sputtering power is 27 watts, sputtering time is 2.5 hours, to magnetron sputtering coating system
The volume flow for the argon gas being passed through in sputtering chamber is 45sccm.
4. 3. substrate that step is obtained is completely immersed in organic solvent, the base 3. obtained using organic solvent dissolving step
Photoresist on material, while also having taken away the Ge above photoresist15Ga10Te75When Chalcogenide films, recycle ultrasonic wave clear
It washes 5 minutes, forms the full sulphur system optical waveguide of Te base.
In this particular embodiment, organic solvent is the N-Methyl pyrrolidone that concentration is 99.9%.
Fig. 2 gives the Ge measured using infrared ellipsometer24Sb3Se73Chalcogenide films and Ge15Ga10Te75Chalcogenide films are each
From refractive index and wavelength relation curve.From figure 2 it can be seen that Ge24Sb3Se73Chalcogenide films and Ge15Ga10Te75Sulphur system
The respective refractive index of film is all gradually reduced with the increase of wavelength, and the two refractive index has apparent difference, shows
Ge24Sb3Se73Chalcogenide films and Ge15Ga10Te75Chalcogenide films are suitble to the production of optical waveguide.
Fig. 3 gives to be illustrated using the result that the method for the present invention prepares per stage during the full sulphur system optical waveguide of Te base
Scheme, 1 is chalcogenide glass in Fig. 3, and 2 be Ge-Sb-Se Chalcogenide films, and 4 be photoresist, and 3 be Ge15Ga10Te75Chalcogenide films.
In above-mentioned each embodiment, the thickness of photoresist has no effect on the property of the full sulphur system optical waveguide of the Te base being prepared
Can, thickness generally usually drips several drops on Ge-Sb-Se Chalcogenide films in 1.5 microns, operation, then whirl coating, protects
Card is uniform.
Below in conjunction with theory, the full sulphur system optical waveguide structure of Te base that aforementioned four different embodiment is prepared is carried out
Analysis:
Table 1 gives the full sulphur system optical waveguide structure of the Te base being prepared under different condition and relevant parameter, including sulphur system
Glass (Chg) substrate material, Ge-Sb-Se Chalcogenide films material and thickness and Ge15Ga10Te75The thickness of Chalcogenide films.
The full sulphur system optical waveguide structure of the Te base being prepared under 1 different condition of table and relevant parameter
Fig. 4 gives the cross-sectional view for the full sulphur system optical waveguide structure of Te base that embodiment one is prepared, W1 in Fig. 4
=4 microns, H1=1 microns, H2=1.2 microns.
Fig. 5 a, which gives, exists to Te base shown in Fig. 4 full sulphur system optical waveguide progress emulation experiment using existing simulation software
Wavelength is the mode distributions figure that obtained TE mould is simulated at 4.8 microns；Fig. 5 b gives using existing simulation software to Fig. 4 institute
It is the mode distributions figure that obtained TM mould is simulated at 4.8 microns that the full sulphur system optical waveguide of the Te base shown, which carries out emulation experiment in wavelength,.
The main integrated distribution of electric field be can be seen that from Fig. 5 a and Fig. 5 b in the central part of waveguide, and do not revealed, sufficiently shown
The full sulphur system optical waveguide structure of the Te base that the method for the present invention is prepared is relatively good, thus the Te base that the method for the present invention is prepared is complete
Sulphur system optical waveguide structure is for realizing that a small electric field effective area provides a good light field restriction effect.
Description of the invention and application be it is illustrative, be not wishing to the scope of the present invention being only restricted in above-described embodiment
In.In the case where not departing from spirit and essential characteristics of the invention, the present invention can otherwise, similar material and group
Distribution ratio is realized.Without departing from the scope and spirit of the present invention, it can be carried out to embodiments disclosed herein
He deforms and changes.
Claims (8)
1. a kind of preparation method of the full sulphur system optical waveguide of Te base, it is characterised in that the following steps are included:
1. taking one piece of chalcogenide glass as substrate；Then plating sets one layer of Ge-Sb-Se sulphur on the smooth upper surface of chalcogenide glass
It is film；Then a layer photoresist is coated on Ge-Sb-Se Chalcogenide films；
The step 1. in the platings of Ge-Sb-Se Chalcogenide films set using magnetically controlled sputter method, wherein magnetron sputtering membrane system
The vacuum degree of the sputtering chamber of system is 1.5 × 10-4Pa~2.5 × 10-4Pa, build-up of luminance air pressure are 2.8 pas~3.2 pas, magnetron sputtering
The sputtering pressure of coating system is 0.22 pa~0.27 pa, sputtering power is 25 watts~30 watts, sputtering time be 2 hours~
3 hours, the volume flow for the argon gas being passed through into the sputtering chamber of magnetron sputtering coating system was 45sccm~55sccm；
2. 1. substrate that step obtains is exposed and is developed using the mask plate with required mask structure, obtains having and cover
The substrate of membrane structure；
3. plating sets one layer of Ge on the 2. substrate with mask structure that step obtains15Ga10Te75Chalcogenide films；
The step 3. in Ge15Ga10Te75The plating of Chalcogenide films is set using magnetically controlled sputter method, wherein magnetron sputtering plating
The vacuum degree of the sputtering chamber of system is 1.5 × 10-4Pa~2.5 × 10-4Pa, build-up of luminance air pressure are 2.8 pas~3.2 pas, and magnetic control splashes
The sputtering pressure for penetrating coating system is 0.22 pa~0.27 pa, sputtering power is 25 watts~30 watts, sputtering time is 2 hours
~3 hours, the volume flow for the argon gas being passed through into the sputtering chamber of magnetron sputtering coating system was 45sccm~55sccm；
4. 3. substrate that step is obtained is completely immersed in organic solvent, in the substrate 3. obtained using organic solvent dissolving step
Photoresist, while taking away the Ge above photoresist15Ga10Te75Chalcogenide films form the full sulphur system optical waveguide of Te base.
2. a kind of preparation method of the full sulphur system optical waveguide of Te base according to claim 1, it is characterised in that the step
The upper and lower surfaces of chalcogenide glass in 1. be by polishing, polishing technology formed smooth surface.
3. a kind of preparation method of the full sulphur system optical waveguide of Te base according to claim 1, it is characterised in that the step
Before 1. plating sets one layer of Ge-Sb-Se Chalcogenide films on the smooth upper surface of chalcogenide glass in, first chalcogenide glass is carried out clear
It washes to go deimpurity pollution, detailed process are as follows: 1. -1, by chalcogenide glass it is completely immersed in acetone, it is then clear using ultrasonic wave
It washes 15 minutes~25 minutes, to remove the impurity on chalcogenide glass；1. -2, the sulphur system glass after taking out cleaning for the first time in acetone
Glass, and the chalcogenide glass of taking-up is completely immersed in methanol, it then utilizes ultrasonic cleaning 3 minutes~8 minutes, tentatively to remove
Remaining acetone on chalcogenide glass；1. -3, from taken out in methanol second clean after chalcogenide glass, and by the sulphur system glass of taking-up
Glass is completely immersed in isopropanol, is then utilized ultrasonic cleaning 3 minutes~8 minutes, remaining on chalcogenide glass to completely remove
Acetone；1. the chalcogenide glass cleaned up -4, is taken out from isopropanol, then with being dried with nitrogen the chalcogenide glass cleaned up.
4. a kind of preparation method of the full sulphur system optical waveguide of Te base according to claim 1, it is characterised in that the step
1. the coating of middle photoresist utilizes sol evenning machine, wherein fast-turn construction after the slow-speed of sol evenning machine elder generation, slow-speed revolving speed are 2000rpm, slow-speed time
It is 3 seconds, fast-turn construction revolving speed is 6000rpm, and the fast-turn construction time is 30 seconds.
5. a kind of preparation method of the full sulphur system optical waveguide of Te base according to claim 1, it is characterised in that the step
Ge-Sb-Se Chalcogenide films in 1. with a thickness of 0.8~1.2 micron, photoresist with a thickness of 1.5~1.8 microns.
6. a kind of preparation method of the full sulphur system optical waveguide of Te base according to claim 4, it is characterised in that the step
2. detailed process are as follows: it is 2. -1, using contact system, right after the photoresist that mask plate is close in 1. substrate that step obtains
1. substrate that step obtains is exposed, wherein the time for exposure is 8 seconds~12 seconds；2. -2, in Sodium Hydroxide Alkaline developer solution
Develop to the substrate after exposure, obtain the substrate with mask structure, wherein developing time is 45 seconds~60 seconds.
7. a kind of preparation method of the full sulphur system optical waveguide of Te base according to claim 1, it is characterised in that the step
Ge in 3.15Ga10Te75Chalcogenide films with a thickness of 0.8~1.2 micron.
8. a kind of preparation method of the full sulphur system optical waveguide of Te base according to claim 1, it is characterised in that the step
The photoresist on substrate for utilizing organic solvent dissolving step 3. to obtain in 4., while taking away above photoresist
Ge15Ga10Te75It is recycled ultrasonic cleaning 5 minutes~10 minutes after Chalcogenide films；The step 4. in organic solvent be
The N-Methyl pyrrolidone that concentration is 99.9%.
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| CN108793738B (en) * | 2018-07-31 | 2021-12-07 | 清远聚航光学材料有限公司 | Optical film and preparation method thereof |
| CN110488416A (en) * | 2019-07-24 | 2019-11-22 | 苏州辰睿光电有限公司 | A method of making small line width rib waveguide |
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